摘要
为应对既往二苯二硫醚合成时存在的体系繁杂、循环及碘回收难度大等问题,决定改进工艺,用SO2/I2/H2O替代SO2/KI/H2SO4/H2O,有机试剂取代水作溶剂。苯磺酰氯∶水∶碘(物质的量比)为20∶10∶1,反应温度60℃,时间6h,选用乙二醇二甲醚作为溶剂。优化工艺下提纯以后目标产物收率、纯度分别是95.9%、99.1%,碘、溶剂的回收率分别为78.6%、82.3%。历经数次循环后,实验结果始终没有出现明显波动,证实了该工艺方案的适用性。
in order to deal with the problems in the synthesis of diphenyl disulfide,such as complex system,difficulty in recycling and iodine recovery,it was decided to improve the process by using SO2/I2/H2 O instead of SO2/ki/H2 SO4/H2 O,and organic reagent instead of water as solvent.The above problems were solved one by one.The mole ratio of benzene sulfonyl chloride to water:iodine was 20:10:1,the reaction temperature was 60℃,and the time was 6 h.The yield and purity of the target product were 95.9%and 99.1%,respectively.The recovery of iodine and solvent were 78.6%and 82.3%,respectively.After several cycles,the experimental results did not fluctuate obviously,which confirmed the applicability of the process.
作者
王杰
Wang Jie(School of Chemistry and Chemical Engineering,Yan'an University,Shaanxi Yan'an 716000)
出处
《云南化工》
CAS
2020年第12期48-50,共3页
Yunnan Chemical Technology
关键词
二苯二硫醚
工艺优化
循环反应
diphenyl disulfide
process optimization
cyclic reaction
